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Combining Capillary Electrochromatography with Ion Trap Accumulation and Time-of-Flight Mass Spectrometry

机译:将毛细管电色谱与离子阱累积和飞行时间质谱相结合

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摘要

Capillary electrochromatography (CEC) is a rapidly developing liquid chromatographic technique in which electroosmotic flow (EOF) is used to propel mobile phase through the chromatographic column. The use of EOF results in reduced band dispersion when compared with pressurised flow, but narrow capillaries are required to avoid dispersion due to heating that arises from the required application of high electrical potentials. Measurement of UV absorbance in these narrow capillaries is therefore relatively insensitive, demanding improved detection methods. This work presents an alternative strategy that is based on the combination of ion trap accumulation with time-of-flight mass spectrometry.ududElectrospray is most often used to transfer analytes from solution to the gas phase, concomitant with ionisation, when interfacing CEC to mass spectrometry. The small volumetric flow rates encountered in CEC, however, raise the possibility of other types of interface being effective. The work presented here describes the development of a novel interface in which a pulsed IR laser is used to vaporise chromatographic eluent, followed by ionisation using a pulsed UV laser. Vaporisation and ionisation both occur within the ion trap to remove the possibility of transmission losses. Ionisation laser wavelength is varied to impart a degree of selectivity. The presence of vaporised solvent and analyte ions inside the trap offers the possibility of performing ion-molecule chemistry.ududIn developing this instrument, the electrochromatographic column was separated from the interface by an electrically grounded junction and a transfer capillary. To preserve chromatographic efficiency, the fluid dynamics of this junction between the column and the transfer capillary were investigated both computationally and experimentally. Simulations of the fluid dynamics of the junction are presented. In order to test the interface without the intermittent, chromatographic, delivery of analyte, a continuous leak inlet was employed. The performance of the instrument was evaluated with polycyclic aromatic hydrocarbons because they are important environmental pollutants and because they are amenable to laser ionisation at 266 nm. Expressed as a number of theoretical plates per metre, an average chromatographic efficiency of 95,000 was obtained with a test mixture that consisted of acenaphthene, biphenyl, fluorene, naphthalene and phenanthrene. Furthermore, using the leak inlet, naphthalene was detected as a 100 nM solution in acetonitrile.
机译:毛细管电色谱(CEC)是一种快速发展的液相色谱技术,其中电渗流(EOF)用于推动流动相通过色谱柱。与加压流相比,使用EOF会导致带扩散减小,但是需要使用狭窄的毛细管来避免由于高电位施加所需的热量而引起的扩散。因此,在这些狭窄的毛细管中测量紫外线吸收率相对不灵敏,需要改进的检测方法。这项工作提出了一种基于离子阱累积与飞行时间质谱相结合的替代策略。 ud ud电喷雾最常用于将分析物从溶液转移到气相,并在与CEC连接时伴随电离质谱分析。但是,在CEC中遇到的体积流量很小,这就增加了其他类型的界面有效的可能性。此处介绍的工作描述了新型界面的开发,其中使用了脉冲IR激光来蒸发色谱洗脱液,然后使用脉冲UV激光进行电离。汽化和电离都在离子阱内发生,以消除传输损失的可能性。改变电离激光波长以赋予一定程度的选择性。捕集阱内蒸发溶剂和分析物离子的存在提供了进行离子分子化学的可能性。 ud ud在开发该仪器时,电色谱柱通过电接地的结点和传输毛细管与界面分离。为了保持色谱效率,在计算和实验上都研究了色谱柱与转移毛细管之间连接处的流体动力学。提出了对接头流体动力学的仿真。为了测试界面时没有分析物的间歇色谱分离,使用了连续的泄漏入口。用多环芳烃评估了仪器的性能,因为它们是重要的环境污染物,并且易于在266 nm激光电离。用每米理论塔板数表示,使用由mixture,联苯,芴,萘和菲组成的测试混合物,平均色谱效率为95,000。此外,使用检漏口检测到萘为100 nM的乙腈溶液。

著录项

  • 作者

    Simpson David C;

  • 作者单位
  • 年度 2003
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  • 原文格式 PDF
  • 正文语种 {"code":"en","name":"English","id":9}
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